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#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/99/4329963.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4329963
loop_
_publ_author_name
'Jan Tillmann'
'Frank Meyer-Wegner'
'Andor Nadj'
'Johanna Becker-Baldus'
'Tanja Sinke'
'Michael Bolte'
'Max C. Holthausen'
'Matthias Wagner'
'Hans-Wolfram Lerner'
_publ_section_title
;
 Unexpected Disproportionation of Tetramethylethylenediamine-Supported
 Perchlorodisilane Cl3SiSiCl3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8599
_journal_page_last               8606
_journal_paper_doi               10.1021/ic301283m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Cl12 Si6, 2(C7 H19 N2), 2(Cl)'
_chemical_formula_sum            'C14 H38 Cl14 N4 Si6'
_chemical_formula_weight         927.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.913(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1630(8)
_cell_length_b                   10.4876(10)
_cell_length_c                   18.4868(16)
_cell_measurement_reflns_used    17905
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.3
_cell_volume                     1946.6(3)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'Genix 3D multilayer optics'
_diffrn_radiation_source         'Genix 3D I\mS microfocus x-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23116
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         3.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.7546
_exptl_absorpt_correction_T_min  0.7388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²+0.3151P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                2859
_reflns_number_total             3652
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic301283m_si_001_3.cif
_cod_data_source_block           wa1401
_cod_database_code               4329963
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cl1 Cl 0.41620(10) 0.90073(11) 0.56806(6) 0.0275(3) Uani 1 1 d .
Si1 Si 0.43830(12) 0.84802(13) 0.40854(7) 0.0271(3) Uani 1 1 d .
Si2 Si 0.63997(12) 0.83281(12) 0.48607(7) 0.0232(3) Uani 1 1 d .
Si3 Si 0.70249(12) 0.98184(12) 0.57817(7) 0.0243(3) Uani 1 1 d .
Cl11 Cl 0.47735(15) 0.84415(16) 0.30172(7) 0.0501(4) Uani 1 1 d .
Cl12 Cl 0.33326(13) 0.67951(12) 0.41483(9) 0.0476(4) Uani 1 1 d .
Cl21 Cl 0.79086(12) 0.82410(13) 0.42235(7) 0.0372(3) Uani 1 1 d .
Cl22 Cl 0.64838(12) 0.65216(11) 0.53278(7) 0.0330(3) Uani 1 1 d .
Cl31 Cl 0.88663(11) 1.05537(13) 0.56616(8) 0.0390(3) Uani 1 1 d .
Cl32 Cl 0.74388(13) 0.88542(12) 0.67730(7) 0.0390(3) Uani 1 1 d .
N1 N 0.0983(4) 0.6045(4) 0.6326(2) 0.0364(10) Uani 1 1 d .
N2 N 0.3970(4) 0.5952(4) 0.7043(2) 0.0309(9) Uani 1 1 d .
C1 C 0.2000(5) 0.5236(6) 0.6090(3) 0.0399(13) Uani 1 1 d .
H1A H 0.1765 0.5094 0.5557 0.048 Uiso 1 1 calc R
H1B H 0.1974 0.4397 0.6333 0.048 Uiso 1 1 calc R
C2 C 0.3405(5) 0.5733(5) 0.6243(3) 0.0343(11) Uani 1 1 d .
H2A H 0.3441 0.6549 0.5978 0.041 Uiso 1 1 calc R
H2B H 0.3990 0.5122 0.6037 0.041 Uiso 1 1 calc R
C11 C -0.0252(6) 0.5304(7) 0.6296(4) 0.0573(17) Uani 1 1 d .
H11A H -0.0944 0.5839 0.6455 0.086 Uiso 1 1 calc R
H11B H -0.0088 0.4562 0.6620 0.086 Uiso 1 1 calc R
H11C H -0.0548 0.5015 0.5793 0.086 Uiso 1 1 calc R
C12 C 0.0741(6) 0.7173(7) 0.5872(4) 0.0603(18) Uani 1 1 d .
H12A H 0.0056 0.7697 0.6047 0.090 Uiso 1 1 calc R
H12B H 0.0435 0.6919 0.5364 0.090 Uiso 1 1 calc R
H12C H 0.1566 0.7665 0.5899 0.090 Uiso 1 1 calc R
C21 C 0.3449(6) 0.7160(5) 0.7314(3) 0.0401(12) Uani 1 1 d .
H21A H 0.3654 0.7871 0.7006 0.060 Uiso 1 1 calc R
H21B H 0.3869 0.7310 0.7820 0.060 Uiso 1 1 calc R
H21C H 0.2482 0.7094 0.7293 0.060 Uiso 1 1 calc R
C22 C 0.3654(6) 0.4873(6) 0.7510(3) 0.0468(15) Uani 1 1 d .
H22A H 0.3990 0.4076 0.7331 0.070 Uiso 1 1 calc R
H22B H 0.2686 0.4813 0.7491 0.070 Uiso 1 1 calc R
H22C H 0.4076 0.5020 0.8017 0.070 Uiso 1 1 calc R
C23 C 0.5458(5) 0.6081(7) 0.7097(3) 0.0482(14) Uani 1 1 d .
H23A H 0.5825 0.5297 0.6919 0.072 Uiso 1 1 calc R
H23B H 0.5851 0.6225 0.7608 0.072 Uiso 1 1 calc R
H23C H 0.5665 0.6804 0.6798 0.072 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl11 Si1 Cl12 102.27(9) . .
Cl11 Si1 Si2 107.83(7) . .
Cl12 Si1 Si2 108.65(8) . .
Cl11 Si1 Si3 109.12(8) . 3_676
Cl12 Si1 Si3 108.49(7) . 3_676
Si2 Si1 Si3 119.17(7) . 3_676
Cl21 Si2 Cl22 102.08(7) . .
Cl21 Si2 Si1 108.21(7) . .
Cl22 Si2 Si1 107.17(7) . .
Cl21 Si2 Si3 107.64(7) . .
Cl22 Si2 Si3 108.63(7) . .
Si1 Si2 Si3 121.44(7) . .
Cl31 Si3 Cl32 102.31(7) . .
Cl31 Si3 Si1 107.90(7) . 3_676
Cl32 Si3 Si1 108.92(8) . 3_676
Cl31 Si3 Si2 108.73(8) . .
Cl32 Si3 Si2 108.27(7) . .
Si1 Si3 Si2 119.37(6) 3_676 .
C12 N1 C1 111.6(5) . .
C12 N1 C11 110.0(5) . .
C1 N1 C11 108.8(5) . .
C22 N2 C21 109.3(4) . .
C22 N2 C23 109.5(4) . .
C21 N2 C23 107.9(4) . .
C22 N2 C2 111.6(4) . .
C21 N2 C2 110.9(4) . .
C23 N2 C2 107.6(4) . .
N1 C1 C2 116.1(4) . .
N1 C1 H1A 108.3 . .
C2 C1 H1A 108.3 . .
N1 C1 H1B 108.3 . .
C2 C1 H1B 108.3 . .
H1A C1 H1B 107.4 . .
C1 C2 N2 116.1(4) . .
C1 C2 H2A 108.3 . .
N2 C2 H2A 108.3 . .
C1 C2 H2B 108.3 . .
N2 C2 H2B 108.3 . .
H2A C2 H2B 107.4 . .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N1 C12 H12A 109.5 . .
N1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N2 C21 H21A 109.5 . .
N2 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
N2 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
N2 C22 H22A 109.5 . .
N2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
N2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
N2 C23 H23A 109.5 . .
N2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
N2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Cl11 2.074(2) .
Si1 Cl12 2.0772(19) .
Si1 Si2 2.3174(17) .
Si1 Si3 2.3239(18) 3_676
Si2 Cl21 2.0754(18) .
Si2 Cl22 2.0783(17) .
Si2 Si3 2.3260(18) .
Si3 Cl31 2.0676(17) .
Si3 Cl32 2.0783(18) .
Si3 Si1 2.3239(18) 3_676
N1 C12 1.448(8) .
N1 C1 1.455(7) .
N1 C11 1.470(7) .
N2 C22 1.489(7) .
N2 C21 1.489(7) .
N2 C23 1.506(7) .
N2 C2 1.518(6) .
C1 C2 1.505(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cl11 Si1 Si2 Cl21 1.09(10) . .
Cl12 Si1 Si2 Cl21 111.22(9) . .
Si3 Si1 Si2 Cl21 -123.91(9) 3_676 .
Cl11 Si1 Si2 Cl22 -108.31(9) . .
Cl12 Si1 Si2 Cl22 1.82(10) . .
Si3 Si1 Si2 Cl22 126.69(8) 3_676 .
Cl11 Si1 Si2 Si3 126.18(9) . .
Cl12 Si1 Si2 Si3 -123.69(9) . .
Si3 Si1 Si2 Si3 1.18(13) 3_676 .
Cl21 Si2 Si3 Cl31 -0.12(9) . .
Cl22 Si2 Si3 Cl31 109.69(8) . .
Si1 Si2 Si3 Cl31 -125.47(8) . .
Cl21 Si2 Si3 Cl32 -110.55(8) . .
Cl22 Si2 Si3 Cl32 -0.74(10) . .
Si1 Si2 Si3 Cl32 124.09(8) . .
Cl21 Si2 Si3 Si1 124.17(8) . 3_676
Cl22 Si2 Si3 Si1 -126.03(8) . 3_676
Si1 Si2 Si3 Si1 -1.19(13) . 3_676
C12 N1 C1 C2 71.5(6) . .
C11 N1 C1 C2 -166.9(5) . .
N1 C1 C2 N2 60.8(7) . .
C22 N2 C2 C1 44.2(6) . .
C21 N2 C2 C1 -77.9(6) . .
C23 N2 C2 C1 164.3(5) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137633
